참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 반응물 | 2-Chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine | HCID 19935587 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 3,4-Dimethoxycarbonyl-2-methoxy-5-nitro-6-phenylpyridine | HCID 19935618 | — |
반응 단계
In 25 ml of methanol was dissolved 1.2 g of 2-chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine as obtained in Reference Example 18. To the solution was added 6.34 ml (2.0 eq.) of a solution of 1N sodium methoxide in methanol, and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was neutralized with 0.2 ml (1.1 eq.) of acetic acid, and the solvent was distilled off. Water was added to the residue, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried. The solvent was distilled off. The residue was purified by silica gel column chromatography (eluent:ethyl acetate). The resulting crystals were collected by filtration with hexane.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05420275 |
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| 출처 데이터셋 | uspto-grants-1995_05 |
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| ORD ID | ord-80287ea4dd174b418b35ca7cef4f89ef |
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| 출처 메모 | uspto-grants-1995_05 |
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